首页> 中文期刊> 《分析测试学报》 >超高效液相色谱-三重四极杆质谱法测定保健食品中30种非法添加壮阳类化合物

超高效液相色谱-三重四极杆质谱法测定保健食品中30种非法添加壮阳类化合物

         

摘要

建立了超高效液相色谱-三重四极杆质谱测定保健食品中30种壮阳类化合物的方法.采用Waters CORTECS T3色谱柱(100 mm×2.1 mm,2.7 μm),以0.1%(体积分数)甲酸水溶液-含0.1%(体积分数)甲酸的乙腈溶液为流动相,梯度洗脱,在电喷雾离子化正离子模式下,以多反应监测模式(MRM)检测.30种化合物在10~ 200 μg/L范围内均呈良好的线性关系,相关系数均大于0.99;在0.1、0.2、1.0 mg/kg加标水平下的平均加标回收率为62.8% ~ 135.2%,相对标准偏差均不大于14%(n=6);检出限为0.05 mg/kg,定量下限为0.1 mg/kg.该方法定性定量准确,操作简便,可为国家标准的建立提供参考.%An analytical method was developed for the determination of 30 anti-impotence compounds illegally adulterated in health products by ultra high performance liquid chromatography-triple quadrupole mass spectrometry(UHPLC-MS/MS) with a Waters CORTECS T3(100 mm ×2.1 mm,2.7 μm) column using 0.1% (by volume) fomic acid aqueous solution-acetonitrile containing 0.1% (by volume) formic acid as mobile phases by gradient elution.The compounds were detected with electrospray ion source in positive mode under multiple reaction monitoring (MRM) mode.The calibration curves for 30 targeted compounds were linear in the mass concentration range of 10-200 μg/L with correlation coefficients more than 0.99.The mean recoveries at spiked levels of 0.1,0.2,1.0 mg/ kg were in the range of 62.8%-135.2%,with RSDs(n =6) not more than 14%.The limits of detection(LODs) and the limits of quantitation(LOQs) were 0.05 mg/kg and 0.1 mg/kg,respectively.The established method is accurate and simple,and could be used as a reference for the national standard.

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